CN116482013A - Experimental device and experimental method for measuring permeation behavior of gaseous or gas-liquid mixed state high-pressure hydrogen - Google Patents
Experimental device and experimental method for measuring permeation behavior of gaseous or gas-liquid mixed state high-pressure hydrogen Download PDFInfo
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- CN116482013A CN116482013A CN202310189225.5A CN202310189225A CN116482013A CN 116482013 A CN116482013 A CN 116482013A CN 202310189225 A CN202310189225 A CN 202310189225A CN 116482013 A CN116482013 A CN 116482013A
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 63
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 63
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000007788 liquid Substances 0.000 title claims abstract description 25
- 238000002474 experimental method Methods 0.000 title claims description 12
- 239000007789 gas Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000010998 test method Methods 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 20
- 229910052759 nickel Inorganic materials 0.000 claims description 18
- 238000007747 plating Methods 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 11
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 10
- 229910052697 platinum Inorganic materials 0.000 claims description 10
- 238000005259 measurement Methods 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 9
- 238000009434 installation Methods 0.000 claims description 6
- 230000000903 blocking effect Effects 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 230000010287 polarization Effects 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000002699 waste material Substances 0.000 claims description 3
- 238000004891 communication Methods 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 16
- 239000003345 natural gas Substances 0.000 abstract description 8
- 238000013461 design Methods 0.000 abstract description 4
- 230000006399 behavior Effects 0.000 description 16
- 229910000831 Steel Inorganic materials 0.000 description 11
- 239000010959 steel Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 238000009826 distribution Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000009662 stress testing Methods 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/02—Electrochemical measuring systems for weathering, corrosion or corrosion-protection measurement
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N13/04—Investigating osmotic effects
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Environmental Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Ecology (AREA)
- Biodiversity & Conservation Biology (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention relates to an experimental device for measuring the permeation behavior of gaseous or gas-liquid mixed state high-pressure hydrogen and a test method thereof, wherein the experimental device for measuring the permeation behavior of gaseous or gas-liquid mixed state high-pressure hydrogen comprises an autoclave, a clamping sleeve joint, a pressure reducing valve, an exhaust valve, a high-pressure hydrogen cylinder, a connecting device of the autoclave and an electrolytic cell, the electrolytic cell, an experimental electrode, an electrochemical workstation and a strain gauge tester; the middle position of the kettle cover at the upper side of the high-pressure kettle is provided with two threaded through holes, the two threaded through holes are respectively connected with a clamping sleeve joint, the clamping sleeve joint is connected with a guide pipe, the two guide pipes are respectively connected with a pressure reducing valve and an exhaust valve, and the pressure reducing valve is connected with a high-pressure gas cylinder through another guide pipe; the invention provides corresponding experimental technical support for pipe selection, process design and safety management of a natural gas hydrogen-adding conveying pipeline by changing the conditions of gas components, gas partial pressure, gas-liquid mixing and the like.
Description
Technical Field
The invention belongs to an experimental device for testing hydrogen permeation behaviors, and particularly relates to an experimental device and an experimental method for measuring high-pressure hydrogen permeation behaviors in a gaseous state or a gas-liquid mixed state.
Background
At present, a plurality of countries in the world develop hydrogen storage and transportation and utilization technologies, and in the existing hydrogen energy storage and transportation technologies, the existing natural gas pipe network is utilized to transport hydrogen in the form of hydrogen-doped natural gas, so that the economy is the most achieved; in the key technology of hydrogen pipeline transportation, pipe evaluation is a research foundation, is a key for evaluating the hydrogen-doped transportation compatibility of a natural gas pipeline, and can cause performance degradation and even failure of pipeline steel in a hydrogen-adjacent environment, hydrogen molecules in the pipeline collide with the surface of steel and are adsorbed on the surface of the steel, and then the hydrogen molecules infiltrate into the steel in an atomic form, so that the pipeline steel is subjected to hydrogen damage phenomena such as hydrogen embrittlement, hydrogen induced cracking, hydrogen bubbling and the like, and the pipeline is cracked, thereby causing gas leakage and even explosion and affecting the safety and property safety along the line; the performance of the gas pipeline and the matched materials under the high-pressure hydrogen gas mixture is an important factor for determining the transportation of the hydrogen-doped natural gas.
At present, the research on the hydrogen embrittlement problem of pipeline steel is mostly carried out in a liquid-phase hydrogen charging environment, and the hydrogen permeation behavior under the actual working condition is difficult to truly reflect due to the fact that the mechanism of entering hydrogen into steel in the liquid-phase hydrogen charging environment and the high-pressure hydrogen environment are different.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide an experimental device and a method for measuring the permeation behavior of gaseous or gas-liquid mixed state high pressure hydrogen, wherein the experimental device for measuring the permeation behavior of gaseous or gas-liquid mixed state high pressure hydrogen can provide corresponding experimental technical support for pipe selection, process design and safety management of natural gas hydrogen-doped conveying pipelines.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention relates to an experimental device for measuring the permeation behavior of gaseous or gas-liquid mixed state high-pressure hydrogen, which is characterized in that: the device comprises an autoclave, a clamping sleeve connector, a pressure reducing valve, an exhaust valve, a high-pressure hydrogen cylinder, a connecting device of the autoclave and an electrolytic cell, the electrolytic cell, an experimental electrode, an electrochemical workstation and a strain gauge tester;
the middle position of the kettle cover at the upper side of the high-pressure kettle is provided with two threaded through holes, the two threaded through holes are respectively connected with a clamping sleeve joint, the clamping sleeve joint is connected with a guide pipe, the two guide pipes are respectively connected with a pressure reducing valve and an exhaust valve, and the pressure reducing valve is connected with a high-pressure gas cylinder through another guide pipe; the middle part of the autoclave body is provided with a circular channel, the outlet end of the circular channel is connected with a connecting device with a central channel, the connecting device is divided into two parts which are detachably connected, a first part of the connecting device is connected with the circular channel of the autoclave, a second part of the connecting device is connected with an electrolytic cell, the first part of the connecting device is provided with a first sink, the second part of the connecting device is provided with a first boss matched with the first sink, the bottom of the first sink is provided with a first gasket and a sample, one side of the sample is provided with an electroplated layer, a strain gauge is connected on the electroplated layer, and the strain gauge is electrically connected with a strain gauge tester positioned outside the connecting device, wherein the side surface of the sample with the electroplated layer faces the electrolytic cell;
a second sinking groove is arranged on the second part of the connecting device, a second boss matched with the second sinking groove is arranged on the electrolytic cell, and a second gasket is arranged in the second sinking groove and used for blocking the electrolytic cell from being communicated with the central channel;
the electrolytic cell is internally provided with a solution and an experimental electrode, and the extending end of the experimental electrode is electrically connected with the electrochemical workstation.
Further, the circular channel is provided with an internal thread, and the convex column of the first part of the connecting device is provided with an external thread in threaded connection with the internal thread of the circular channel.
Further, the first portion and the second portion of the connecting device are locked and fixed by bolts.
Further, the first gasket and the second gasket are made of polytetrafluoroethylene materials.
Further, the autoclave and the autoclave cover are made of stainless steel materials, the autoclave cover is connected with the autoclave in an embedded connection mode, the inner diameter of the autoclave is one hundred millimeters, and the height of the inner space of the autoclave is two hundred millimeters.
Further, the clamping sleeve joint is connected with the autoclave cover through threads, and sealing is added by thread glue.
Further, the experimental electrodes are platinum electrodes and saturated calomel electrodes.
The invention relates to a test method for measuring the permeation behavior of gaseous or gas-liquid mixed state high-pressure hydrogen, which is characterized by comprising the following steps of:
the method comprises the following steps:
step one: simulating different working conditions, and adopting different hydrogen concentrations;
step two: polishing two sides of a sample, carrying out nickel plating treatment on a hydrogen measurement surface of the sample by using an electrochemical workstation, and sticking strain gauges on the nickel plating surface after nickel plating is finished;
step three: placing a first gasket at the bottom of a first sinking groove of the connecting device, placing a sample adhered with a strain gauge on one side of the first gasket close to the autoclave, wherein the surface of the sample, which is not plated with nickel, faces the autoclave, fixing a first part and a second part of the connecting device with bolts and nuts to achieve the purpose of fixing the first gasket and the sample, purging the autoclave with nitrogen of 1MPa for 3 times after the installation is completed, exhausting air in the autoclave, and finally performing air tightness test on the autoclave with nitrogen;
step four: the strain gauge is connected to a strain gauge tester through a wire, and 0.5 mol/LH is added into an autoclave according to the experimental requirements 2 SO 4 The stress values on the nickel plating surface of the sample are measured by a strain gauge tester, wherein the pressure of the solution or pure hydrogen is 1MPa, 3MPa, 5MPa, 7MPa and 10MPa respectively;
step five: after the stress measurement experiment is completed, an exhaust valve is opened, tail gas is treated, then a sample which is used for the experiment before the sample which is subjected to nickel plating treatment but is not adhered with a strain gauge is replaced is used, after the installation is completed, the autoclave is purged 3 times by nitrogen with the pressure of 1MPa, air in the autoclave is discharged, and finally the air tightness of the autoclave is inspected by the nitrogen;
step six, a step of performing a step of; after the air tightness test is finished, connecting the electrolytic cell with a connecting device, placing a second gasket in a second precipitation tank to prevent the solution from exuding, adding 0.1 mol/LNaOH solution into the electrolytic cell, placing a platinum electrode and a saturated calomel electrode into the solution, respectively connecting the platinum electrode serving as an auxiliary electrode, the saturated calomel electrode serving as a reference electrode and a sample serving as a working electrode with an electrochemical workstation, opening the electrochemical workstation to start anodic polarization, and reducing background current;
step seven: after the background current is reduced to meet the experimental requirement and stabilized, adding 0.5 mol/LH into the autoclave according to the experimental requirement 2 SO 4 The pressure of the solution and the nitrogen or the pure hydrogen is respectively 1MPa, 3MPa, 5MPa, 7MPa and 10MPa;
step eight: after the hydrogen permeation current measurement experiment is finished, an exhaust valve is opened, tail gas is treated, the waste liquid treated by the electrolytic cell is taken down, and a sample is taken out.
The invention is an experimental device which can simulate the pipeline steel hydrogen permeation behavior under different hydrogen-loading working conditions by changing the conditions of gas components, gas partial pressure, gas-liquid mixing and the like, simulate the pipeline steel hydrogen permeation behavior of a pipe under different hydrogen-loading working conditions, measure the stress distribution of a material through a strain gauge system, analyze the influence of different hydrogen-loading working conditions on the material hydrogen permeation behavior through electrochemical experimental results, and provide corresponding experimental technical support for the pipe selection, process design and safety management of a natural gas hydrogen-loading conveying pipeline.
Drawings
FIG. 1 is a schematic diagram of an experimental set-up of the present invention;
FIG. 2 is a schematic view of an autoclave during stress testing;
FIG. 3 is an enlarged view of a portion of the connection device during stress testing;
FIG. 4 is a schematic view of an autoclave during hydrogen permeation testing;
FIG. 5 is an enlarged view of a portion of the connection device during hydrogen permeation testing;
FIG. 6 is a schematic illustration of strain gauge attachment;
the marks in the figure are in turn: 1. a high pressure gas cylinder; 2. a pressure reducing valve; 3. an exhaust valve; 4. a ferrule joint; 5. an autoclave; 6. a connecting device; 7. an electrolytic cell; 8. a platinum electrode; 9. a saturated calomel electrode; 10. an electrochemical workstation; 11. an O-ring; 12. a first gasket; 13. a strain gage; 14. a sample; 15. a second gasket;
601. a first portion; 602. A second portion; 603. A first sink; 604. A first boss; 605. A second sink; 606. a second boss; 501 internal threads.
Detailed Description
The invention will be further described with reference to the accompanying drawings and examples.
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the present application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
The experimental device for measuring the permeation behavior of the gaseous or gas-liquid mixed state high-pressure hydrogen comprises an autoclave 5, a clamping sleeve connector 4, a pressure reducing valve 2, an exhaust valve 3, a high-pressure hydrogen cylinder 1, a connecting device 6 of the autoclave and an electrolytic cell, the electrolytic cell 7, an experimental electrode, an electrochemical workstation 10 and a strain gauge tester (not shown in the figure).
Two threaded through holes are formed in the middle of the kettle cover on the upper side of the autoclave 5, the two threaded through holes are respectively connected with a clamping sleeve joint 4, and the clamping sleeve joint is connected with the autoclave cover through threads and is additionally sealed by thread glue; the cutting sleeve joint is connected with a guide pipe, the two guide pipes are respectively connected with a pressure reducing valve 2 and an exhaust valve 3, and the pressure reducing valve 2 is connected with the high-pressure gas cylinder 1 through another guide pipe; the middle part of the autoclave body 5 is provided with a circular channel, the outlet end of the circular channel is connected with a connecting device 6 with a central channel, the connecting device 6 is divided into two parts which are detachably connected, namely a first part 601 and a second part 602 of the connecting device, and the first part 601 and the second part 602 are locked and fixed through bolts.
The first part 601 of the connection device is connected with the circular channel of the autoclave (the circular channel is provided with an internal thread 501, the convex column of the first part of the connection device is provided with an external thread connected with the internal thread of the circular channel, the convex column of the first part of the connection device is provided with an O-shaped ring 11, the second part 602 of the connection device is connected with the electrolytic cell 7, the first part of the connection device is provided with a first sinking groove 603, the second part of the connection device is provided with a first boss 604 matched with the first sinking groove, the bottom of the first sinking groove is provided with a first gasket 12 and a sample 14, one side of the sample is provided with a plating layer, the plating layer is connected with a strain gauge 13, and the strain gauge is electrically connected with a strain gauge tester positioned outside the connection device, wherein the side of the sample with the plating layer faces the electrolytic cell.
A second sink 605 is provided on the second part of the connection device, a second boss 606 is provided on the electrolytic cell, which mates with the second sink, and a second gasket 15 is provided in the second sink for blocking the communication between the electrolytic cell and the central passage.
The electrolytic cell is internally provided with a solution, a platinum electrode and a saturated calomel electrode, and the extending end of the experimental electrode is electrically connected with the electrochemical workstation.
Specifically, the first gasket and the second gasket are made of polytetrafluoroethylene materials, the autoclave and the autoclave cover are made of stainless steel materials, the autoclave cover is connected with the autoclave in an embedded connection mode, the inner diameter of the autoclave is one hundred millimeters, and the height of the inner space is two hundred millimeters.
The invention relates to a test method for measuring the permeation behavior of high-pressure hydrogen in a gaseous state or a gas-liquid mixed state,
the method comprises the following steps:
step one: simulating different working conditions, and adopting different hydrogen concentrations;
step two: polishing two sides of a sample, carrying out nickel plating treatment on a hydrogen measurement surface of the sample by using an electrochemical workstation, and sticking strain gauges on the nickel plating surface after nickel plating is finished;
step three: placing a first gasket at the bottom of a first sinking groove of the connecting device, placing a sample adhered with a strain gauge on one side of the first gasket close to the autoclave, wherein the surface of the sample, which is not plated with nickel, faces the autoclave, fixing a first part and a second part of the connecting device with bolts and nuts to achieve the purpose of fixing the first gasket and the sample, purging the autoclave with nitrogen of 1MPa for 3 times after the installation is completed, exhausting air in the autoclave, and finally performing air tightness test on the autoclave with nitrogen;
step four: the strain gauge is connected to a strain gauge tester through a wire, and 0.5 mol/LH is added into an autoclave according to the experimental requirements 2 SO 4 The stress values on the nickel plating surface of the sample are measured by a strain gauge tester, wherein the pressure of the solution or pure hydrogen is 1MPa, 3MPa, 5MPa, 7MPa and 10MPa respectively;
step five: after the stress measurement experiment is completed, an exhaust valve is opened, tail gas is treated, then a sample which is used for the experiment before the sample which is subjected to nickel plating treatment but is not adhered with a strain gauge is replaced is used, after the installation is completed, the autoclave is purged 3 times by nitrogen with the pressure of 1MPa, air in the autoclave is discharged, and finally the air tightness of the autoclave is inspected by the nitrogen;
step six, a step of performing a step of; after the air tightness test is finished, connecting the electrolytic cell with a connecting device, placing a second gasket in a second precipitation tank to prevent the solution from exuding, adding 0.1 mol/LNaOH solution into the electrolytic cell, placing a platinum electrode and a saturated calomel electrode into the solution, respectively connecting the platinum electrode serving as an auxiliary electrode, the saturated calomel electrode serving as a reference electrode and a sample serving as a working electrode with an electrochemical workstation, opening the electrochemical workstation to start anodic polarization, and reducing background current;
step seven: after the background current is reduced to meet the experimental requirement and stabilized, adding 0.5 mol/LH into the autoclave according to the experimental requirement 2 SO 4 The pressure of the solution and the nitrogen or the pure hydrogen is respectively 1MPa, 3MPa, 5MPa, 7MPa and 10MPa;
step eight: after the hydrogen permeation current measurement experiment is finished, an exhaust valve is opened, tail gas is treated, the waste liquid treated by the electrolytic cell is taken down, and a sample is taken out.
The invention is an experimental device which can simulate the pipeline steel hydrogen permeation behavior under different hydrogen-loading working conditions by changing the conditions of gas components, gas partial pressure, gas-liquid mixing and the like, simulate the pipeline steel hydrogen permeation behavior of a pipe under different hydrogen-loading working conditions, measure the stress distribution of a material through a strain gauge system, analyze the influence of different hydrogen-loading working conditions on the material hydrogen permeation behavior through electrochemical experimental results, and provide corresponding experimental technical support for the pipe selection, process design and safety management of a natural gas hydrogen-loading conveying pipeline.
The above-described embodiments are provided to further explain the objects, technical solutions, and advantageous effects of the present invention in detail. It should be understood that the foregoing is only illustrative of the present invention and is not intended to limit the scope of the present invention. It should be noted that any modifications, equivalent substitutions, improvements, etc. made by those skilled in the art without departing from the spirit and principles of the present invention are intended to be included in the scope of the present invention.
Claims (8)
1. An experimental device for measuring gaseous or gas-liquid mixed state high pressure hydrogen permeation behavior, which is characterized in that: the device comprises an autoclave (5), a clamping sleeve joint (4), a pressure reducing valve (2), an exhaust valve (3), a high-pressure hydrogen cylinder (1), a connecting device (6) of the autoclave and an electrolytic cell, the electrolytic cell (7), an experimental electrode, an electrochemical workstation (10) and a strain gauge tester;
two threaded through holes are formed in the middle of a kettle cover on the upper side of the high-pressure kettle (5), the two threaded through holes are respectively connected with a clamping sleeve joint (4), the clamping sleeve joint is connected with a guide pipe, the two guide pipes are respectively connected with a pressure reducing valve (2) and an exhaust valve (3), and the pressure reducing valve (2) is connected with a high-pressure gas cylinder (1) through another guide pipe; the middle part of the autoclave body of the autoclave (5) is provided with a circular channel, the outlet end of the circular channel is connected with a connecting device (6) with a central channel, the connecting device (6) is divided into two parts which are detachably connected, a first part (601) of the connecting device is connected with the circular channel of the autoclave, a second part (602) of the connecting device is connected with an electrolytic cell (7), the first part of the connecting device is provided with a first sink (603), the second part of the connecting device is provided with a first boss (604) matched with the first sink, a first gasket (12) and a sample (14) are placed at the bottom of the first sink, one side of the sample is provided with an electroplated layer, a strain gauge (13) is connected on the electroplated layer, the strain gauge is electrically connected with a strain gauge tester positioned outside the connecting device, and the side surface of the sample provided with the electroplated layer faces the electrolytic cell;
a second sinking groove (605) is arranged on the second part of the connecting device, a second boss (606) matched with the second sinking groove is arranged on the electrolytic cell, and a second gasket (15) is arranged in the second sinking groove and used for blocking the communication between the electrolytic cell and the central channel;
the electrolytic cell is internally provided with a solution and an experimental electrode, and the extending end of the experimental electrode is electrically connected with the electrochemical workstation.
2. The experimental device for measuring the permeation behavior of gaseous or gas-liquid mixed state high pressure hydrogen according to claim 1, wherein: the circular channel is provided with an internal thread (501), the convex column of the first part of the connecting device is provided with an external thread in threaded connection with the internal thread of the circular channel, and the convex column of the first part of the connecting device is provided with an O-shaped ring (11).
3. The experimental device for measuring the permeation behavior of gaseous or gas-liquid mixed state high pressure hydrogen according to claim 1, wherein: the first part (601) and the second part (602) of the connecting device are locked and fixed through bolts.
4. The experimental device for measuring the permeation behavior of gaseous or gas-liquid mixed state high pressure hydrogen according to claim 1, wherein: the first and second washers are constructed of polytetrafluoroethylene material.
5. The experimental device for measuring the permeation behavior of gaseous or gas-liquid mixed state high pressure hydrogen according to claim 1, wherein: the autoclave and the autoclave cover are made of stainless steel materials, the autoclave cover is connected with the autoclave in an embedded connection mode, the inner diameter of the autoclave is one hundred millimeters, and the height of the inner space of the autoclave is two hundred millimeters.
6. The experimental device for measuring the permeation behavior of gaseous or gas-liquid mixed state high pressure hydrogen according to claim 1, wherein: the clamping sleeve joint is connected with the autoclave cover through threads, and is additionally sealed by thread glue.
7. The experimental device for measuring the permeation behavior of gaseous or gas-liquid mixed state high pressure hydrogen according to claim 1, wherein: the experimental electrode is a platinum electrode and a saturated calomel electrode.
8. A test method for measuring the permeation behaviour of gaseous or gas-liquid mixed state high pressure hydrogen as claimed in any one of claims 1 to 7, wherein:
the method comprises the following steps:
step one: simulating different working conditions, and adopting different hydrogen concentrations;
step two: polishing two sides of a sample, carrying out nickel plating treatment on a hydrogen measurement surface of the sample by using an electrochemical workstation, and sticking strain gauges on the nickel plating surface after nickel plating is finished;
step three: placing a first gasket at the bottom of a first sinking groove of the connecting device, placing a sample adhered with a strain gauge on one side of the first gasket close to the autoclave, wherein the surface of the sample, which is not plated with nickel, faces the autoclave, fixing a first part and a second part of the connecting device with bolts and nuts to achieve the purpose of fixing the first gasket and the sample, purging the autoclave with nitrogen of 1MPa for 3 times after the installation is completed, exhausting air in the autoclave, and finally performing air tightness test on the autoclave with nitrogen;
step four: the strain gauge is connected to a strain gauge tester through a wire, and 0.5 mol/LH is added into an autoclave according to the experimental requirements 2 SO 4 The stress values on the nickel plating surface of the sample are measured by a strain gauge tester, wherein the pressure of the solution or pure hydrogen is 1MPa, 3MPa, 5MPa, 7MPa and 10MPa respectively;
step five: after the stress measurement experiment is completed, an exhaust valve is opened, tail gas is treated, then a sample which is used for the experiment before the sample which is subjected to nickel plating treatment but is not adhered with a strain gauge is replaced is used, after the installation is completed, the autoclave is purged 3 times by nitrogen with the pressure of 1MPa, air in the autoclave is discharged, and finally the air tightness of the autoclave is inspected by the nitrogen;
step six, a step of performing a step of; after the air tightness test is finished, connecting the electrolytic cell with a connecting device, placing a second gasket in a second precipitation tank to prevent the solution from exuding, adding 0.1 mol/LNaOH solution into the electrolytic cell, placing a platinum electrode and a saturated calomel electrode into the solution, respectively connecting the platinum electrode serving as an auxiliary electrode, the saturated calomel electrode serving as a reference electrode and a sample serving as a working electrode with an electrochemical workstation, opening the electrochemical workstation to start anodic polarization, and reducing background current;
step seven: after the background current is reduced to meet the experimental requirement and stabilized, adding 0.5 mol/LH into the autoclave according to the experimental requirement 2 SO 4 The pressure of the solution and the nitrogen or the pure hydrogen is respectively 1MPa, 3MPa, 5MPa, 7MPa and 10MPa;
step eight: after the hydrogen permeation current measurement experiment is finished, an exhaust valve is opened, tail gas is treated, the waste liquid treated by the electrolytic cell is taken down, and a sample is taken out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| CN117554245A (en) * | 2024-01-11 | 2024-02-13 | 中国航发北京航空材料研究院 | Device and method for measuring hydrogen diffusion coefficient of nickel-based superalloy based on resistivity |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117554245A (en) * | 2024-01-11 | 2024-02-13 | 中国航发北京航空材料研究院 | Device and method for measuring hydrogen diffusion coefficient of nickel-based superalloy based on resistivity |
| CN117554245B (en) * | 2024-01-11 | 2024-03-26 | 中国航发北京航空材料研究院 | Device and method for measuring hydrogen diffusion coefficient of nickel-based superalloy based on resistivity |
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